Polyaniline–chitosan (PAni–Cs) composite films were synthesized using a solution casting method with varying PAni concentrations. Polyaniline powders used in the composite synthesis were polymerized using acetic acid as the dopant media. Raman spectroscopy revealed that the PAni powders synthesized using hydrochloric acid and acetic acid did not exhibit significant difference to the chemical features of PAni, implying that PAni was formed in varying concentrations of the dopant media. The presence of agglomerated particles on the surface of the Cs composite, which may have been due to the presence of PAni powders, was observed with scanning electron microscope–energy dispersive X-ray spectroscopy (SEM–EDX). Ultraviolet–visible (UV–Vis) spectroscopy further showed the interaction of PAni with Cs where the Cs characteristic peak shifted to a higher wavelength. Cell viability assay also revealed that the synthesized PAni–Cs composites were nontoxic and may be utilized for future biomedical applications.